DE19503060A1 - Cleaning procedure for membrane filters - Google Patents
Cleaning procedure for membrane filtersInfo
- Publication number
- DE19503060A1 DE19503060A1 DE19503060A DE19503060A DE19503060A1 DE 19503060 A1 DE19503060 A1 DE 19503060A1 DE 19503060 A DE19503060 A DE 19503060A DE 19503060 A DE19503060 A DE 19503060A DE 19503060 A1 DE19503060 A1 DE 19503060A1
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- Prior art keywords
- cleaning
- solution
- membranes
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- membrane
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D41/00—Regeneration of the filtering material or filter elements outside the filter for liquid or gaseous fluids
- B01D41/04—Regeneration of the filtering material or filter elements outside the filter for liquid or gaseous fluids of rigid self-supporting filtering material
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/042—Acids
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38636—Preparations containing enzymes, e.g. protease or amylase containing enzymes other than protease, amylase, lipase, cellulase, oxidase or reductase
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38645—Preparations containing enzymes, e.g. protease or amylase containing cellulase
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/39—Organic or inorganic per-compounds
- C11D3/3947—Liquid compositions
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
- C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
- C12H1/02—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material
- C12H1/06—Precipitation by physical means, e.g. by irradiation, vibrations
- C12H1/063—Separation by filtration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/16—Use of chemical agents
- B01D2321/164—Use of bases
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/16—Use of chemical agents
- B01D2321/166—Use of enzymatic agents
Abstract
Description
Die Erfindung betrifft ein enzymatisches Verfahren zur Reinigung von Membranen, insbesondere von Membranen zur Mikrofiltration, die in Brauereien zur Filtration von Bier verwendet werden. Durch das erfindungsgemäße Reinigungsverfahren werden Verblockungen der Mem bran beseitigt, so daß zur Klarfiltration von Bier auf ökonomische Weise Mikrofiltrationsmembranen verwendet werden können. Hierdurch kann die bisher übliche Filtration über Kieselgur, die nach Ende der Gebrauchsdauer als Abfall beseitigt werden muß, durch eine we sentlich abfallärmere Membranfiltration ersetzt werden.The invention relates to an enzymatic process for cleaning of membranes, in particular membranes for microfiltration, the used in breweries for the filtration of beer. By the cleaning method according to the invention will block the mem bran eliminated so that for the clear filtration of beer on economical Way microfiltration membranes can be used. Hereby Filtration through diatomaceous earth, which is common at the end of the day the service life must be disposed of as waste by a we Substantially less waste membrane filtration can be replaced.
In Brauereien werden verstärkt Membranfiltrationsanlagen zu unter schiedlichen Zwecken eingesetzt. Beispielsweise genannt seien: 1) Kaltsterilisation von Bier mit Dead-End-Mikrofiltrationsmembranen direkt vor dem Füller, 2) Aufbereitung von Heferestbier sowie Rückbier mit Cross-Flow-Mikrofiltration und 3) Klarfiltration von Bier mit Cross-Flow-Mikrofiltration anstelle der Kieselgurfiltra tion (befindet sich noch im Versuchsstadium).In breweries, membrane filtration systems are increasingly becoming too used for different purposes. Examples include: 1) Cold sterilization of beer with dead-end microfiltration membranes directly in front of the filler, 2) preparation of residual yeast beer as well Back beer with cross-flow microfiltration and 3) clear filtration of Beer with cross-flow microfiltration instead of the diatomaceous earth filter tion (is still in the experimental stage).
Bisher ist es praktisch nicht möglich, die beispielsweise aus Polypropylen bestehenden Filtermaterialien so zu reinigen, daß ein reibungsloser Betriebsablauf auf Dauer gewährleistet ist. Die Mem branen unterliegen unterschiedlichen Verblockungsursachen. Zum ei nen bildet sich auf den Membranen eine Deckschicht, die zu Lei stungsverlusten führt. Diese Deckschicht kann durch eine klassische Reinigung entfernt werden. Daneben findet aber auch zum anderen eine innere Verblockung der Membranporen statt, die bislang als irreversibel angesehen wurde. Dies äußert sich in einem kontinu ierlichen Druckanstieg oder in einer Leistungsreduzierung der Mem branen. Besonders bei der oben unter 3) genannten Klarfiltration fällt die mit zunehmender Membranverblockung einhergehende Pro duktveränderung wie beispielsweise Aufhellung des Biers und Ent fernung von Aromastoffen unangenehm ins Gewicht. Die Verblockung kann aus einer sogenannten Primärverblockung bestehen, bei der Trübstoffe, Hefereste etc. auf der Membran abgelagert werden. Diese Art der Verblockung ist konventionell entfernbar. Weiterhin kann eine sogenannte Sekundärverblockung der Poren eintreten, die von Bierinhaltsstoffen hervorgerufen wird, die in den Poren der Membran adsorbieren. Hierbei kann es sich um Glucane, höhere Alkohole, Ester sowie Wachse, Polyphenole und Polysaccharide handeln. Diese Art der Porenverblockung kann nun erstmals mit dem erfindungsgemäßen Verfahren rückgängig gemacht werden.So far it is practically not possible, for example, from Polypropylene to clean existing filter materials so that a smooth operation is guaranteed in the long run. The mem industries are subject to different causes of blocking. To the egg NEN, a top layer forms on the membranes, which leads to lei loss of performance. This top layer can be replaced by a classic Cleaning can be removed. In addition, it also finds another an internal blocking of the membrane pores, which was previously known as was considered irreversible. This manifests itself in a continuous or a decrease in performance of the mem branches. Especially with the clear filtration mentioned under 3) falls the pro associated with increasing membrane blockage Product changes such as brightening the beer and Ent Removal of aromas uncomfortable in weight. The blocking can consist of a so-called primary blocking, in which Turbidities, yeast residues etc. are deposited on the membrane. These The type of interlocking can be removed conventionally. Furthermore can a so-called secondary blocking of the pores occurs, which is caused by Beer ingredients are produced in the pores of the membrane adsorb. These can be glucans, higher alcohols, Trade esters as well as waxes, polyphenols and polysaccharides. These The type of pore blocking can now be used for the first time the inventive method can be reversed.
In der Bierbrauerei ist es bekannt, soweit es nationale Regelungen erlauben, dem Bier Enzymmischungen zuzusetzen, die die Aufgabe ha ben, nicht stärkehaltige Polymere wie Glucan, Xylan und Cellulose abzubauen. Hierfür sind Enzymmischungen im Handel, die hauptsäch lich aus β-Glucanase bestehen und Nebenaktivitäten aus Cellulase und Xylanase enthalten. Bei der Klarfiltration des Biers erhöhen solche Enzymzusätze die Filtrationsleistung und führen zu Einspa rungen bei Filterhilfsmitteln. Weiterhin werden Glucan-Nach trübungen verhindert. Zur Membranreinigung wurden derartige Enzyme noch nicht mit Erfolg eingesetzt.In the brewery it is known as far as there are national regulations allow to add enzyme mixtures to the beer that have the task ben, non-starchy polymers such as glucan, xylan and cellulose dismantle. For this, enzyme mixtures are commercially available, the main ones Lich consist of β-glucanase and secondary activities from cellulase and contain xylanase. Increase when clarifying the beer such enzyme additions the filtration performance and lead to savings filter aids. Glucan-Nach prevents turbidity. Such were used for membrane cleaning Enzymes have not yet been used successfully.
Der Erfindung liegt die Aufgabe zugrunde, ein Reinigungsverfahren für Filtrationsmembranen, insbesondere für Membranen zur Mikrofil tration, bereitzustellen, mit dem die bei der Filtration von Bier auftretenden Verblockungen beseitigt werden können.The invention has for its object a cleaning method for filtration membranes, especially for microfilm membranes tration to provide with which in the filtration of beer blockages that occur can be eliminated.
Diese Aufgabe wird gelöst durch ein Verfahren zum Reinigen von Filtrationsmembranen für die Bierfiltration, dadurch gekennzeich net, daß man zumindest folgende Schritte ausführt:This object is achieved by a method for cleaning Filtration membranes for beer filtration, characterized net that you carry out at least the following steps:
- a) Behandlung der Membran mit einer enzymhaltigen wäßrigen Lösung, wobei als Enzyme β-Glucanasen, Xylanasen und Cellulasen einge setzt werden,a) treating the membrane with an enzyme-containing aqueous solution, being used as enzymes β-glucanases, xylanases and cellulases be put
- b) Reinigung mit einer sauren wäßrigen Reinigungslösung,b) cleaning with an acidic aqueous cleaning solution,
- c) Reinigung mit einer peroxidhaltigen alkalischen Reinigungslö sung.c) Cleaning with an alkaline cleaning solution containing peroxide solution.
Dabei ist es vorzuziehen, vor und nach jedem der einzelnen Teil schritte mit Wasser zu spülen.It is preferable to do this before and after each part steps to rinse with water.
Die im Teilschritt a) einsetzbare Enzymmischung, die vorzugsweise β-Glucanasen als Hauptkomponenten und Xylanasen und Cellulasen als Nebenkomponenten enthält, ist in der Brautechnik als Bierzusatz zur Verbesserung des Filtrationsverhaltens bekannt. Für den erfindungsgemäßen Einsatz zur Reinigung von Filtrationsmembranen enthält die Lösung vorzugsweise 0,5 bis 3 Gew.-% Enzyme. Weiterhin ist es bevorzugt, daß die wäßrige Enzymlösung außerdem 2 bis 10 Gew.-% Alkalimetall- und/oder Ammoniumphosphate, insbesondere in der Form der Triphosphate, enthält. Weiterhin ist es vorzuziehen, daß die Enzymlösung zur Einstellung des besonders wirksamen pH-Wer tes im Bereich von etwa 4 bis etwa 6 1 bis 10 Gew.-% Carbonsäuren mit nicht mehr als 10 C-Atomen enthält. Hierfür sind Hydroxycarbonsäuren wie beispielsweise Milchsäure, Äpfelsäure, Weinsäure und insbesondere Citronensäure und Gluconsäure bevorzugt. The enzyme mixture that can be used in sub-step a), preferably β-glucanases as main components and xylanases and cellulases as Contains secondary components, is used in brewing technology as a beer additive Improvement in filtration behavior known. For the use according to the invention for cleaning filtration membranes the solution preferably contains 0.5 to 3% by weight of enzymes. Farther it is preferred that the aqueous enzyme solution further 2 to 10 % By weight of alkali metal and / or ammonium phosphates, especially in the form of the triphosphates. Furthermore, it is preferable that the enzyme solution to adjust the particularly effective pH tes in the range of about 4 to about 6 1 to 10 wt .-% Contains carboxylic acids with no more than 10 carbon atoms. For this are Hydroxycarboxylic acids such as lactic acid, malic acid, Tartaric acid and especially citric acid and gluconic acid are preferred.
Die im Teilschritt a) einsetzbare enzymhaltige wäßrige Lösung weist vorzugsweise eine Temperatur zwischen 15 und 50°C auf, wobei die Temperatur beispielsweise bei 25°C liegen kann. Dabei ist es in der Regel ausreichend, die Reinigungslösung etwa eine Stunde lang auf die Membran einwirken zu lassen. Bei sehr stark verblockten Membranen kann jedoch auch eine längere Einwirkungszeit, bei spielsweise von bis zu einer Woche, benötigt werden. Vorzugsweise geht man in diesem Teilschritt a) so vor, daß man zunächst die Konzentratseite der Membran durch kurzzeitiges Überströmen mit der Enzymlösung von einer gebildeten Deckschicht befreit. Diese Lösung verwirft man anschließend. Danach läßt man die Membran von frischer Enzymlösung durchströmen und sie anschließend in dieser Lösung bis zum Ende der erwünschten Einwirkungszeit stehen.The enzyme-containing aqueous solution which can be used in sub-step a) has preferably a temperature between 15 and 50 ° C, the Temperature can be 25 ° C, for example. It is in usually sufficient, the cleaning solution for about an hour to act on the membrane. With very heavily blocked However, membranes can also have a longer exposure time for example up to a week. Preferably one proceeds in this sub-step a) in such a way that the Concentrate side of the membrane by briefly overflowing with the Enzyme layer removed from a top layer formed. This solution then discard. Then the membrane is left fresh Flow through the enzyme solution and then in this solution until at the end of the desired exposure time.
Nach der Einwirkung der wäßrigen Enzymlösung wird die Membran vor zugsweise mit Wasser gespült, wonach sich der erfindungsgemäße Teilschritt b), die Reinigung mit einer sauren wäßrigen Reini gungslösung, anschließt. Hierfür wird vorzugsweise eine saure wäß rige Reinigungslösung eingesetzt, die etwa 0,2 bis etwa 1,0 Gew.-% einer oder mehrerer Mineralsäuren enthält. Die Mineralsäuren sind vorzugsweise ausgewählt aus Salpetersäure und/oder Phosphorsäure. Geeignete Konzentrate solcher Reinigungslösungen sind im Handel erhältlich, beispielsweise unter dem Namen P3-ultrasil®75 der Firma Henkel-Ecolab, Düsseldorf. Beispielsweise kann eine 1 gew.-%ige wäßrige Lösung dieses Handelsprodukts im Teilschritt b) eingesetzt werden. Die Temperatur dieser Reinigungslösung liegt vorzugsweise zwischen 30 und 60°C, beispielsweise bei etwa 50°C. Die saure wäßrige Reinigungslösung soll für einen Zeitraum zwischen 10 und 60 Minuten, beispielsweise für etwa 20 Minuten, auf die Membran ein wirken. After exposure to the aqueous enzyme solution, the membrane is pre preferably rinsed with water, after which the invention Sub-step b), cleaning with an acidic aqueous cleaner solution, connects. For this purpose, an acidic aq cleaning solution that contains about 0.2 to about 1.0% by weight contains one or more mineral acids. The mineral acids are preferably selected from nitric acid and / or phosphoric acid. Suitable concentrates of such cleaning solutions are commercially available available, for example under the name P3-ultrasil®75 from the company Henkel-Ecolab, Düsseldorf. For example, a 1 wt .-% aqueous solution of this commercial product used in substep b) will. The temperature of this cleaning solution is preferably between 30 and 60 ° C, for example at about 50 ° C. The sour one aqueous cleaning solution should last for a period between 10 and 60 Minutes, for example for about 20 minutes, on the membrane Act.
Vorzugsweise folgt auf diesen Teilschritt wieder eine Zwischenspü lung mit Wasser. Der nächste erfindungswesentliche Schritt ist c) die Reinigung mit einer peroxidhaltigen alkalischen Reinigungslö sung. Dabei enthält die alkalische Reinigungslösung vorzugsweise 0,05 bis 0,3 Gew.-% Wasserstoffperoxid. Dies kann als solches oder in Form von Wasserstoffperoxid-abspaltenden Verbindungen wie bei spielsweise Percarbonaten, Perboraten, Peroxosulfaten oder Peroxodisulfaten eingesetzt werden. Dabei wird die Konzentration der Wasserstoffperoxid-abspaltenden Verbindungen so gewählt, daß sich hieraus eine rechnerische Konzentration von 0,05 bis 0,3 Gew.-% Wasserstoffperoxid ergibt. Die Verwendung von Wasserstoff peroxid als solchem ist vorteilhaft. Als Alkalitätsträger enthält die alkalische Reinigungslösung vorzugsweise Alkalimetallhydroxide, wie beispielsweise Natrium- und insbesondere Kalium-hydroxid. Der Gehalt an Alkalimetall-hydroxid kann beispielsweise zwischen 0,1 und 0,5 Gew.-% liegen. Beispielsweise genannt sei ein Gehalt an Kalium-hydroxid von 0,3 Gew.-%. Weitere bevorzugte Komponenten der alkalischen Reinigungslösung sind 0,2 bis 0,5 Gew.-% anionische, nichtionische und/oder zwitterionische Tenside. Als anionische Tenside kommen beispielsweise Alkansulfonate mit C-Kettenlängen von 14 bis 16 in Betracht, als nichtionische Tenside vorzugsweise Ethoxylierungsprodukte von Fettalkoholen mit 12 bis 18 C-Atomen mit 20 bis 35 Ethylenoxidgruppen und als zwitterionische Tenside bei spielsweise Cocosalkylamphocarboxypropionat in Betracht. Weiterhin enthält die alkalische Reinigungslösung vorzugsweise 0,02 bis 0,3 Gew.-% Chelatkomplexbildner wie beispielsweise Phosphonobutantri carbonsäure-salze und/oder Ethylendiamintetraacetat und/oder Ni trilotriacetat. Mit dieser alkalischen Reinigungslösung, die vor zugsweise eine Temperatur im Bereich zwischen 35 und 60°C, bei spielsweise 50°C, aufweist, werden die Membranen im Teilschritt c) für eine Zeitdauer zwischen 10 und 60 Minuten, beispielsweise 20 Minuten, behandelt. Vorzugsweise schließt sich an diese Behandlung eine Spülung mit Wasser an.An intermediate rinse preferably follows this sub-step again with water. The next step essential to the invention is c) cleaning with an alkaline cleaning solution containing peroxide solution. The alkaline cleaning solution preferably contains 0.05 to 0.3 wt% hydrogen peroxide. As such or in the form of compounds releasing hydrogen peroxide as in for example percarbonates, perborates, peroxosulfates or Peroxodisulfates are used. The concentration of the hydrogen peroxide-releasing compounds selected so that this results in a calculated concentration of 0.05 to 0.3 Wt .-% hydrogen peroxide results. The use of hydrogen peroxide as such is advantageous. Contains as an alkalinity carrier the alkaline cleaning solution, preferably alkali metal hydroxides, such as sodium and especially potassium hydroxide. Of the Alkali metal hydroxide content can be, for example, between 0.1 and 0.5% by weight. One example is a content of Potassium hydroxide of 0.3% by weight. Other preferred components of the alkaline cleaning solutions are 0.2 to 0.5% by weight anionic, non-ionic and / or zwitterionic surfactants. As anionic For example, surfactants come from alkanesulfonates with C chain lengths of 14 to 16 into consideration, preferably as nonionic surfactants Ethoxylation products of fatty alcohols with 12 to 18 carbon atoms 20 to 35 ethylene oxide groups and as zwitterionic surfactants for example, coconut alkyl amphocarboxypropionate. Farther the alkaline cleaning solution preferably contains 0.02 to 0.3 % By weight of chelating agents such as, for example, phosphonobutane tri carboxylic acid salts and / or ethylenediaminetetraacetate and / or Ni trilotriacetate. With this alkaline cleaning solution, the before preferably a temperature in the range between 35 and 60 ° C, at for example 50 ° C, the membranes in sub-step c) for a period of between 10 and 60 minutes, for example 20 Minutes, treated. This treatment preferably follows a rinse with water.
Nach diesem Teilschritt c) ist das erfindungsgemäße Reinigungsver fahren abgeschlossen und die Durchgängigkeit der Membran weitgehend wieder hergestellt. Um die Membranen zuverlässig tensidfrei zu wa schen, ist es jedoch vorzuziehen, einen erneuten sauren Reini gungsschritt mit einer tensidfreien Reinigungslösung vorzusehen. Hierfür kann die gleiche saure Reinigungslösung wie im Teilschritt b) verwendet werden, wobei deren Konzentration im Vergleich zu der im Teilschritt b) gewählten halbiert werden kann. Zeitdauer und Temperaturen entsprechen denjenigen des Teilschritts b). Nach die ser sauren Nachbehandlung ist eine erneute Wasserspülung empfeh lenswert.After this sub-step c) is the cleaning process according to the invention drive completed and the patency of the membrane largely restored. To ensure that the membranes are reliably free of surfactants However, it is preferable to do another acidic clean step with a surfactant-free cleaning solution. The same acidic cleaning solution can be used as in the partial step b) are used, their concentration compared to that can be halved in sub-step b). Duration and Temperatures correspond to those of substep b). After the This acidic after-treatment is recommended to flush the water again worth it.
Das erfindungsgemäße Reinigungsverfahren wurde besonders zur Rei nigung von Membranen entwickelt, die zur Mikrofiltration eingesetzt werden. Die Mikrofiltration ist als typisches Membrantrennverfahren im Stand der Technik bekannt. Siehe beispielsweise: Ullmann′s Encyclopedia of Industrial Chemistry, 5. Auflage, 1991, Band 16, SS 194 und 195. Bei der Mikrofiltration werden Membranen aus unter schiedlichen Materialien eingesetzt, die Poren im Größenbereich 0,1 bis 10 Mikrometer aufweisen und die demnach größere Partikel zu rückhalten. Dieser Trennprozeß erfordert üblicherweise eine hydro statische Druckdifferenz über die Membran in der Größenordnung 10 bis 500 kPa.The cleaning method according to the invention was especially for Rei developed membranes used for microfiltration will. Microfiltration is a typical membrane separation process known in the art. See for example: Ullmann’s Encyclopedia of Industrial Chemistry, 5th edition, 1991, volume 16, SS 194 and 195. In microfiltration, membranes are made from under different materials used, the pores in the size range 0.1 have up to 10 microns and the larger particles accordingly hold back. This separation process usually requires a hydro static pressure difference across the membrane in the order of 10 up to 500 kPa.
Für die Anwendung des erfindungsgemäßen Reinigungsverfahrens ist das Membranmaterial nicht kritisch. Beispielsweise ist das Verfah ren für Membranen aus Polypropylen geeignet. Weitere mögliche Mem branmaterialien sind Polysulfon, Polyethersulfon, PVDF, Polyamid und Nylon H66. Aber auch Keramikmembranen wie beispielsweise solche aus Siliciumkarbid, Aluminiumoxid oder Titanoxid sind mit dem erfindungsgemäßen Verfahren zu reinigen. Die Membranen können als Rohrmodule, Plattenmodule oder als Wickelmodule ausgeführt sein.For the application of the cleaning method according to the invention the membrane material is not critical. For example, the process suitable for membranes made of polypropylene. Other possible memes Industry materials are polysulfone, polyether sulfone, PVDF, polyamide and nylon H66. But also ceramic membranes such as those made of silicon carbide, aluminum oxide or titanium oxide are with the to clean the method according to the invention. The membranes can be used as Pipe modules, plate modules or as winding modules.
Durch das erfindungsgemäße Reinigungsverfahren, das man vorzugs weise einmal täglich durchführt, können Verblockungen von Mikro filtrationsmembranen bei der Bierfiltration verhindert bzw. rück gängig gemacht werden. Die hierdurch erzielte verlängerte Membran standzeit erlaubt es, Mikrofiltrationsverfahren für die Klarfil tration von Bier ökonomisch vorteilhaft einzusetzen. Solche Fil trationsverfahren sind daher geeignet, die bisher übliche Filtra tion über Filterhilfsmittel wie beispielsweise Kieselgur, die nach Ende ihrer Gebrauchsdauer als zu entsorgender Müll anfallen, zu ersetzen.By the cleaning method according to the invention, which is preferred wise once a day can block micro filtration membranes prevented or reversed in beer filtration be made common. The elongated membrane achieved in this way service life allows microfiltration processes for the clear film use of beer economically. Such fil trationsverfahren are therefore suitable, the previously common Filtra tion on filter aids such as diatomaceous earth, which after End of their useful life as waste to be disposed of replace.
Das erfindungsgemäße Verfahren wurde an einer Mikrofiltrationsmem bran aus Polypropylen in Form eines Rohrmoduls mit einer Membran fläche von 0,2 m² und 40 m² erprobt, die zuvor durch Klarfiltration von frisch gebrautem Bier zum Verblocken gebracht wurde. Dabei wurden folgende Teilschritte ausgeführt:The method according to the invention was carried out on a microfiltration membrane Bran made of polypropylene in the form of a tubular module with a membrane tested areas of 0.2 m² and 40 m², previously by clear filtration was blocked by freshly brewed beer. Here the following substeps were carried out:
- 1) Ausspülen der Anlage mit Frischwasser;1) rinsing the system with fresh water;
- 2) Reinigung mit einer enzymhaltigen Reinigungslösung gemäß Teil schritt a) für eine Stunde bei 25°C;2) Cleaning with an enzyme-containing cleaning solution according to part step a) for one hour at 25 ° C;
- 3) Zwischenspülung mit Wasser;3) intermediate rinsing with water;
- 4) Reinigung mit einer sauren wäßrigen Reinigungslösung gemäß Teilschritt b) (P3-ultrasil®75, Henkel-Ecolab, Düsseldorf, An satz 1%ig in Wasser) für 20 Minuten bei 50°C;4) Cleaning with an acidic aqueous cleaning solution according to Sub-step b) (P3-ultrasil®75, Henkel-Ecolab, Düsseldorf, An 1% in water) for 20 minutes at 50 ° C;
- 5) Zwischenspülung mit Wasser;5) intermediate rinsing with water;
- 6) Reinigung mit einer peroxidhaltigen alkalischen Reinigungslö sung gemäß Teilschritt c): die wäßrige Lösung enthielt 0,14 Gew.-% H₂O₂, 0,3 Gew.-% Kaliumhydroxid, 0,1 Gew.-% Na₄-Ethylendiamintetraacetat und 0,32 Gew.-% einer Tensidmischung aus nichtionischen, zwitterionischen und anio nischen Tensiden (Ethoxylierungsprodukt von Talgfettalkohol mit ca. 30 Ethylenoxideinheiten, Cocosamphocarboxypropionat und Alkansulfonat im Gewichtsverhältnis 30 : 1 : 1), Einwirkungs dauer 20 Minuten, Temperatur der Lösung 50°C;6) Cleaning with an alkaline cleaning solution containing peroxide solution according to sub-step c): the aqueous solution contained 0.14 % By weight H₂O₂, 0.3% by weight potassium hydroxide, 0.1% by weight Na₄-ethylenediaminetetraacetate and 0.32 wt .-% one Mixture of surfactants from non-ionic, zwitterionic and anio African surfactants (ethoxylation product of tallow fatty alcohol with approx. 30 ethylene oxide units, coco amphocarboxypropionate and Alkanesulfonate in a weight ratio of 30: 1: 1), exposure duration 20 minutes, temperature of the solution 50 ° C;
- 7) Zwischenspülung mit Wasser;7) intermediate rinsing with water;
- 8) saure Nachspülung mit einer Reinigungslösung wie unter 4), je doch mit halbierter Konzentration, Behandlungsdauer 20 Minuten, Temperatur der Lösung 50°C,8) acidic rinsing with a cleaning solution as under 4), each but with halved concentration, treatment time 20 minutes, Temperature of the solution 50 ° C,
- 9) Nachspülen mit Wasser.9) Rinse with water.
Nach dieser Reinigungsfolge war die ursprüngliche Durchlässigkeit der Membran wieder hergestellt. Vergleichsversuche, in denen der erfindungsgemäße Teilschritt a) weggelassen oder mit anderen En zymmischungen, die keine β-Glucanasen, Xylanasen und Cellulasen enthielten, führten nicht zu einer Aufhebung der Membranver blockung.After this cleaning sequence was the original permeability the membrane is restored. Comparative experiments in which the Sub-step a) according to the invention omitted or with other En enzymes that do not contain β-glucanases, xylanases and cellulases contained, did not lead to a cancellation of the membrane ver blocking.
Claims (10)
- a) Behandlung der Membran mit einer enzymhaltigen wäßrigen Lö sung, wobei als Enzyme β-Glucanasen, Xylanasen und Cellulasen eingesetzt werden,
- b) Reinigung mit einer sauren wäßrigen Reinigungslösung,
- c) Reinigung mit einer peroxidhaltigen alkalischen Reinigungs lösung.
- a) treatment of the membrane with an enzyme-containing aqueous solution, β-glucanases, xylanases and cellulases being used as enzymes,
- b) cleaning with an acidic aqueous cleaning solution,
- c) Cleaning with an alkaline cleaning solution containing peroxide.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19503060A DE19503060A1 (en) | 1995-02-01 | 1995-02-01 | Cleaning procedure for membrane filters |
| DE59601608T DE59601608D1 (en) | 1995-02-01 | 1996-01-23 | CLEANING METHOD FOR MEMBRANE FILTERS |
| AT96901322T ATE178500T1 (en) | 1995-02-01 | 1996-01-23 | CLEANING PROCEDURE FOR MEMBRANE FILTER |
| DK96901322T DK0808212T3 (en) | 1995-02-01 | 1996-01-23 | Membrane filter cleaning process |
| PCT/EP1996/000258 WO1996023579A1 (en) | 1995-02-01 | 1996-01-23 | Method of cleaning membrane filters |
| EP96901322A EP0808212B1 (en) | 1995-02-01 | 1996-01-23 | Method of cleaning membrane filters |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19503060A DE19503060A1 (en) | 1995-02-01 | 1995-02-01 | Cleaning procedure for membrane filters |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE19503060A1 true DE19503060A1 (en) | 1996-08-08 |
Family
ID=7752778
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19503060A Withdrawn DE19503060A1 (en) | 1995-02-01 | 1995-02-01 | Cleaning procedure for membrane filters |
| DE59601608T Expired - Lifetime DE59601608D1 (en) | 1995-02-01 | 1996-01-23 | CLEANING METHOD FOR MEMBRANE FILTERS |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE59601608T Expired - Lifetime DE59601608D1 (en) | 1995-02-01 | 1996-01-23 | CLEANING METHOD FOR MEMBRANE FILTERS |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP0808212B1 (en) |
| AT (1) | ATE178500T1 (en) |
| DE (2) | DE19503060A1 (en) |
| DK (1) | DK0808212T3 (en) |
| WO (1) | WO1996023579A1 (en) |
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- 1996-01-23 WO PCT/EP1996/000258 patent/WO1996023579A1/en active IP Right Grant
- 1996-01-23 DE DE59601608T patent/DE59601608D1/en not_active Expired - Lifetime
- 1996-01-23 DK DK96901322T patent/DK0808212T3/en active
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Also Published As
| Publication number | Publication date |
|---|---|
| EP0808212A1 (en) | 1997-11-26 |
| ATE178500T1 (en) | 1999-04-15 |
| DE59601608D1 (en) | 1999-05-12 |
| EP0808212B1 (en) | 1999-04-07 |
| DK0808212T3 (en) | 1999-10-18 |
| WO1996023579A1 (en) | 1996-08-08 |
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| 8139 | Disposal/non-payment of the annual fee |